CN104261818A - High-performance microwave dielectric ceramic material and preparation method thereof - Google Patents
High-performance microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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- CN104261818A CN104261818A CN201410481937.5A CN201410481937A CN104261818A CN 104261818 A CN104261818 A CN 104261818A CN 201410481937 A CN201410481937 A CN 201410481937A CN 104261818 A CN104261818 A CN 104261818A
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Abstract
The invention provides a high-performance microwave dielectric ceramic material which is prepared from xMO-yLn2O3-zTiO2 and a metal nanoscale additive, wherein M comprises Ba and further comprises one or two of Ca or Sr; Ln comprises La and further comprises one or more of Sm, Pm, Nd, Pr or Eu; the metal nanoscale additive comprises Zn and further comprises one or more of Zr, Sn, Mg, Ni, Co or W; and x+y+z is equal to 1. The invention further provides a preparation method of the ceramic material. According to the microwave dielectric ceramic material provided by the invention, the dielectric constant is 46-48, and meanwhile has a relatively high quality factor of 35000-50000GHz, and the temperature coefficient of resonance frequency can be adjusted within a range from -12ppm/DEG C to +12ppm/DEG C.
Description
Technical field
The present invention relates to stupalith field, specifically a kind of high performance microwave medium ceramic material and preparation method thereof.
Background technology
The microwave resonator and the wave filter that are applied to 3G and 4G base station must have good frequency selective characteristic, bandwidth, miniaturization and low cost.Although existing metal cavitg resonator cost is lower, its nonloaded Q very low (~ 6000GHz), and resonant frequency temperature stability is very poor.
Dielectric resonator has that Q-unloaded is high, frequency-temperature coefficient is little and adjustable, the feature such as volume is little usually, is thus subject to applying more and more widely.Corresponding microwave dielectric ceramic materials must have the high quality factor (Q in (1) higher specific inductivity (30-60), (2) simultaneously
f>=40000GHz), (3) nearly zero adjustable temperature coefficient of resonance frequency.
Although the specific inductivity of medium is higher, the size of resonator and wave filter can be less.But the specific inductivity of medium is excessive in this case, in dielectric resonator, electromagnetic field concentrates in medium, causes the coupling of resonator too weak and the bandwidth of wave filter is diminished.And the Q of dielectric material
fvalue and specific inductivity are inversely proportional to, and usual specific inductivity is greater than 60 and its Q of dielectric material of temperature coefficient of resonance frequency nearly zero
fvalue is no more than 30000GHz.
The requirement of development to the quality factor of dielectric material of modern communications industry is more and more higher, the Q of commercialization at present
fthe microwave dielectric material that value is higher mainly contains Ba (Mg
1/3ta
2/3) O
3(BMT), Ba (Zn
1/3ta
2/3) O
3(BZT), LnAlO
3-CaTiO
3system, Zr-Ti-Sn-O system and ZrTiO
4-ZnNb
2o
6system etc., the Q of BMT and BZT in these materials
falthough higher, raw materials used Ta
2o
5expensive, sintering temperature is high; LnAlO
3-CaTiO
3although the sintering temperature of system is lower, Q
fvalue can not meet the development need of industry completely, and the part rare earth prices of raw and semifnished materials are unstable; Zr-Ti-Sn-O system and ZrTiO
4-ZnNb
2o
6the Q of system
falthough higher, specific inductivity is less than normal.In a word, the development trend of current modern communications industry to dielectric material requirement be meet the comparatively large and temperature coefficient of resonance frequency of specific inductivity nearly zero adjustable while, Q to be improved as much as possible
fvalue, will reduce costs, the stability of enhancing product performance and repeatability simultaneously.
Summary of the invention
Main purpose of the present invention is that the deficiency existed for above-mentioned background technology provides a kind of specific inductivity large, Q
fbe worth high, temperature coefficient of resonance frequency is nearly zero adjustable, and cost is low, and is easy to the high performance microwave medium ceramic material produced in enormous quantities.
The present invention is achieved through the following technical solutions: a kind of high performance microwave medium ceramic material, and it is by x MO-y Ln
2o
3-z TiO
2with metal nano level additive composition,
Wherein, M comprises Ba, and Ln comprises La, and metal nano level additive comprises Zn,
The molar content of each component is respectively above:
The molar content of x is 5-35mol/%;
The molar content of y is 10-50mol/%;
The molar content of z is 35-80mol/%;
x+y+z＝1；
The mass percentage of metal nano level additive is 1-5wt/%.
Preferably, M also comprise in Ca or Sr one or both, wherein BaO is 5-35mol/%, CaO be 0-10mol/%, SrO is 0-10mol/%;
Ln also comprise in Sm, Pm, Nd, Pr or Eu one or more, wherein La
2o
3for 10-50mol/%, Sm
2o
3for 0-5mol/%, Pm
2o
3for 0-5mol/%, Nd
2o
3for 0-5mol/%, Pr
2o
3for 0-5mol/%, Eu
2o
3for 0-5mol/%;
Preferably, described metal nano level additive also comprises one or more in Zr, Sn, Mg, Ni, Co or W; Wherein Zn is 1-2.5wt/%, Zr be 0-2wt/%, Sn be 0-1.5wt/%, Mg be 0-1.5wt/%, Ni be 0-1wt/%, Co be 0-0.5wt/%, W is 0-1wt/%.
Another object of the present invention is to provide the preparation method of above-mentioned high performance microwave medium ceramic material.
It is achieved by the following technical solution: a kind of method preparing above-mentioned high performance microwave medium ceramic material, and its step comprises:
(1) MCO is taken by the mol ratio of raw material
3, Ln
2o
3and TiO
2, then add water and zirconium ball, in ball mill, slip is dried after becoming slip by ball milling;
(2) powder after drying is crossed 40 mesh sieves, and at 1000-1200 DEG C, calcine cooling after 3 hours obtain ceramic powder;
(3) pour into adding metal nano level additive in ceramic powder in ball mill, add water and zirconium ball, slip is dried after becoming slip by ball milling again;
(4) in above-mentioned powder, add polyvinyl alcohol solution and carry out granulation, and cross 40 mesh sieves after grinding evenly;
(5) powder after granulation is loaded mould dry-pressing formed under the pressure of 120MPa; Then by the ceramic green after shaping except no-bonder, after finally sintering 2-12 hour with the temperature rise rate of 5 DEG C/min at 1400-1550 DEG C, furnace cooling obtains the high performance microwave medium ceramic material sintered.
Preferably, be that ball milling becomes slip in 24 hours in ball mill in described step (1), then put into baking oven and be dried into powder at 120 DEG C.
Preferably, be that ball milling becomes slip in 24 hours in ball mill in described step (3), then put into baking oven and be dried into powder at 120 DEG C.
Preferably, in described step (3), metal nano level additive is by after metal alkoxide, diethanolamine, alcoholic solvent, water mixing, through the gel metal nanometer additive that hydrolysis, polycondensation obtain.
Preferably, the mass percentage of the polyvinyl alcohol solution added in described step (4) is 10%, and add-on is 7-10%.
Preferably, removing binding agent described in described step (5) is at 800 DEG C be that 5 DEG C/min heats removing in 2 hours with temperature rise rate.
In the above-mentioned methods, MO oxide compound is due to character instability, and general raw material adopts MCO
3form add, the component of actual stupalith exists with MO form.The concrete fineness of the ball milling form slurry in step (1) and (3) is determined according to the character of stupalith, is those skilled in the art's conventional means.
Microwave dielectric ceramic materials of the present invention, its specific inductivity is 46-48, has the quality factor that 35000-50000GHz is higher simultaneously, and temperature coefficient of resonance frequency is adjustable in-12 ppm/ DEG C ~+12ppm/ DEG C.Microwave dielectric ceramic materials of the present invention can be used as the key core material of the electronic devices and components such as microwave mobile communication wave filter, resonator, vibrator and electrical condenser, be widely used in the modern communications industries such as satellite communications, mobile communication, Global Positioning System, Bluetooth technology and WLAN (wireless local area network), there is important industrial application value.
Embodiment
By the following specific examples further illustrate the invention:
Embodiment 1
(1) BaCO that purity is greater than 99.95% is accurately taken
30.11mol, CaCO
30.008mol, La
2o
30.19mol, Sm
2o
30.012mol and TiO
20.42mol, pours in resin balls grinding jar, adds deionized water and zirconium ball; The weight ratio of three is: material: ball: deionized water=1:2:1.5; Ball milling 24 hours in ball mill, to ensure to mix; After discharging, slip is put into baking oven, dry at 120 DEG C and obtain the powder after drying;
(2) powder after oven dry is crossed 40 mesh sieves, calcine 3 hours at 1200 DEG C subsequently, furnace cooling, obtains ceramic powder;
(3) 1wt/% chemical pure zinc alkoxide (Zn) is got and 1.5wt/% chemical pure magnesium alkoxide (Mg) is respectively dissolved in dehydrated alcohol, respectively add appropriate diethanolamine to mix, respectively add deionized water subsequently, by hydrolysis, polycondensation, then form gel, obtained granularity is nano level liquid phase Zn addition material and the Mg addition material of 50-60nm.Wherein above-mentioned alkoxide can be ethanol, ethylene glycol and propyl carbinol.
(4) synthetic ceramic powder is poured in resin balls grinding jar together with nano level liquid phase addition material, add deionized water and zirconium ball; The weight ratio of three is: material: ball: deionized water=1:2:0.75; Ball milling 24 hours in ball mill, to ensure the powder obtaining epigranular about 0.12 μm; After discharging, slip is put into baking oven, dry at 120 DEG C;
(5) concentration adding 7-10Wt% in above-mentioned powder is after the drying the polyvinyl alcohol solution of 10Wt%, carries out granulation, and crosses 40 mesh sieves after grinding evenly in mortar; Powder after granulation is loaded mould is dry-pressing formed under the pressure of 120MPa is
cylinder; Then the right cylinder after shaping is heated at 800 DEG C 2 hours with except no-bonder, its temperature rise rate is 5 DEG C/min, finally at 1400-1550 DEG C, sinter 2-12 hour with identical temperature rise rate, EP (end of program) is closed temperature regulating device furnace cooling and is obtained microwave dielectric ceramic materials 1.
Embodiment 2
BaCO
30.108mol, SrCO
30.008mol, La
2o
30.192mol, Sm
2o
30.0102mol, Pm
2o
30.008mol, TiO
20.418mol, 2wt/% zinc alkoxide (Zn) and 1wt/% nickel alkoxide (Ni).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 2.
Embodiment 3
BaCO
30.118mol, La
2o
30.194mol, Eu
2o
30.0122mol, TiO
20.420mol, 2.5wt/% zinc alkoxide (Zn) and 1wt/% tin alkoxide (Sn).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 3.
Embodiment 4
BaCO
30.112mol, CaCO
30.0036mol, SrCO
30.003mol, La
2o
30.198mol, Sm
2o
30.0112mol, TiO
20.422mol, 2.5wt/% zinc alkoxide (Zn) and 0.5wt/% cobalt alkoxide (Co).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 4.
Embodiment 5
BaCO
30.12mol, La
2o
30.196mol, Eu
2o
30.0122mol, TiO
20.418mol, 2.5wt/% zinc alkoxide (Zn), 1wt/% magnesium alkoxide (Mg) and 1.5wt/% tin alkoxide (Sn).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 5.
Embodiment 6
BaCO
30.0375mol, SrCO
30.0375mol, La
2o
30.375mol, TiO
20.3mol, 2wt/% zinc alkoxide (Zn), 1wt/% zirconium alkoxide (Zr) and 0.3wt/% cobalt alkoxide (Co).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 6.
Embodiment 7
BaCO
30.112mol, CaCO
30.007mol, La
2o
30.195mol, Sm
2o
30.0108mol, Pr
2o
30.0024mol, TiO
20.422mol, 2wt/% zinc alkoxide (Zn), 1wt/% tin alkoxide (Sn) and 1wt/% tungsten alkoxide (W).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 7.
Embodiment 8
BaCO
30.114mol, CaCO
30.002mol, SrCO
30.004mol, La
2o
30.198mol, Nd
2o
30.01mol, TiO
20.416mol, 1wt/% zinc alkoxide (Zn), 1wt/% magnesium alkoxide (Mg) and 0.5wt/% tungsten alkoxide (W).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 8.
Embodiment 9
BaCO
30.115mol, SrCO
30.004mol, La
2o
30.195mol, Eu
2o
30.002mol, Pr
2o
30.002mol, TiO
20.418mol, 1wt/% zinc alkoxide (Zn), 1wt/% tin alkoxide (Sn), 1wt/% magnesium alkoxide (Mg), 1wt/% cobalt alkoxide (Co).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 9.
Embodiment 10
BaCO
30.114mol, CaCO
30.007mol, La
2o
30.188mol, Nd
2o
30.008mol, Eu
2o
30.012mol, TiO
20.422mol, 1wt/% zinc alkoxide (Zn), 0.5wt/% nickel alkoxide (Ni), 1wt/% magnesium alkoxide (Mg), 0.5wt/% tungsten alkoxide (W).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 10.
Embodiment 11
BaCO
30.0375mol, La
2o
30.225mol, Sm
2o
30.0375mol, Pr
2o
30.0375mol, Nd
2o
30.0375mol, Eu
2o
30.0375mol, TiO
20.3375mol, 1wt/% zinc alkoxide (Zn), 2wt/% zirconium alkoxide (Zr), 1wt/%mol tin alkoxide (Sn), 1wt/% nickel alkoxide (Ni).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 11.
Embodiment 12
BaCO
30.1125mol, CaCO
30.075mol, SrCO
30.075mol, La
2o
30.075mol, TiO
20.4125mol, 1wt/% zinc alkoxide (Zn).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 12.
Embodiment 13
BaCO
30.2625mol, La
2o
30.1875mol, Pm
2o
30.0375mol, TiO
20.2625mol, 1wt/% zinc alkoxide (Zn).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 13.
Embodiment 14
BaCO
30.075mol, La
2o
30.075mol, TiO
20.6mol, 1wt/% zinc alkoxide (Zn).Preparation method is identical with embodiment 1, obtains microwave dielectric ceramic materials 14.
Adopt Hakki-Coleman method, under 3GHz frequency, to the specific inductivity of the microwave dielectric ceramic materials of embodiment 1-14, Q
fvalue and temperature coefficient of resonance frequency are tested, and test result is as shown in table 1.
Table 1 microwave dielectric ceramic materials 1-15 performance.
Claims (9)
1. a high performance microwave medium ceramic material, it is by x MO-y Ln
2o
3-z TiO
2with metal nano level additive composition,
Wherein, M comprises Ba, and Ln comprises La, and metal nano level additive comprises Zn,
The molar content of each component is respectively above:
The molar content of x is 5-35mol/%;
The molar content of y is 10-50mol/%;
The molar content of z is 35-80mol/%;
x+y+z＝1；
The mass percentage of metal nano level additive is 1-5wt/%.
2. a kind of high performance microwave medium ceramic material according to claim 1, is characterized in that: M also comprise in Ca or Sr one or both, wherein BaO is 5-35mol/%, CaO be 0-10mol/%, SrO is 0-10mol/%;
Ln also comprise in Sm, Pm, Nd, Pr or Eu one or more, wherein La
2o
3for 10-50mol/%, Sm
2o
3for 0-5mol/%, Pm
2o
3for 0-5mol/%, Nd
2o
3for 0-5mol/%, Pr
2o
3for 0-5mol/%, Eu
2o
3for 0-5mol/%.
3. a kind of high performance microwave medium ceramic material according to claim 1 and 2, is characterized in that: described metal nano level additive also comprise in Zr, Sn, Mg, Ni, Co or W one or more; Wherein Zn is 1-2.5wt/%, Zr be 0-2wt/%, Sn be 0-1.5wt/%, Mg be 0-1.5wt/%, Ni be 0-1wt/%, Co be 0-0.5wt/%, W is 0-1wt/%.
4. prepare a method for high performance microwave medium ceramic material described in claim 1, its step comprises:
(1) MCO is taken by the mol ratio of raw materials
3, Ln
2o
3and TiO
2, then add water and zirconium ball, in ball mill, slip is dried after becoming slip by ball milling;
(2) powder after drying is crossed 40 mesh sieves, and at 1000-1200 DEG C, calcine cooling after 3 hours obtain ceramic powder;
(3) pour into adding metal nano level additive in ceramic powder in ball mill, add water and zirconium ball, slip is dried after becoming slip by ball milling again;
(4) in above-mentioned powder, add polyvinyl alcohol solution and carry out granulation, and cross 40 mesh sieves after grinding evenly;
(5) powder after granulation is loaded mould dry-pressing formed under the pressure of 120MPa; Then by the ceramic green after shaping except no-bonder, after finally sintering 2-12 hour with the temperature rise rate of 5 DEG C/min at 1400-1550 DEG C, furnace cooling obtains the high performance microwave medium ceramic material sintered.
5. the preparation method of high performance microwave medium ceramic material according to claim 2, is characterized in that: be that ball milling becomes slip in 24 hours in ball mill in described step (1), then put into baking oven and be dried into powder at 120 DEG C.
6. the preparation method of high performance microwave medium ceramic material according to claim 2, is characterized in that: be that ball milling becomes slip in 24 hours in ball mill in described step (3), then put into baking oven and be dried into powder at 120 DEG C.
7. the preparation method of high performance microwave medium ceramic material according to claim 2, it is characterized in that: in described step (3), metal nano level additive is by after metal alkoxide, diethanolamine, alcoholic solvent, water mixing, through the gel metal nanometer additive that hydrolysis, polycondensation obtain.
8. the preparation method of high performance microwave medium ceramic material according to claim 2, is characterized in that: the mass percentage of the polyvinyl alcohol solution added in described step (4) is 10%, and add-on is 7-10%.
9. the preparation method of high performance microwave medium ceramic material according to claim 2, is characterized in that: removing binding agent described in described step (5) is at 800 DEG C be that 5 DEG C/min heats removing in 2 hours with temperature rise rate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198426A (en) * | 2015-09-07 | 2015-12-30 | 桂林理工大学 | Temperature stable ultra-low dielectric constant microwave dielectric ceramic SmYV2O8 |
| CN111377709A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material, dielectric ceramic block and microwave communication equipment |
| CN111377731A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material and preparation method of dielectric ceramic block |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105198426A (en) * | 2015-09-07 | 2015-12-30 | 桂林理工大学 | Temperature stable ultra-low dielectric constant microwave dielectric ceramic SmYV2O8 |
| CN111377709A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material, dielectric ceramic block and microwave communication equipment |
| CN111377731A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Microwave dielectric ceramic material and preparation method of dielectric ceramic block |
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Application publication date: 20150107 |